Extrusion-grade polyarylene sulfide bar and preparation method thereof
A polyarylene sulfide, extrusion-grade technology, applied in the field of polymer synthesis, can solve the requirements of high viscosity and high melt strength of single-screw extruded rods or profiles, and it is difficult to extrude to prepare high-strength and high-strength materials. Tough polyphenylene sulfide profiles, insufficient melt viscosity and melt strength, etc., achieve the effects of excellent mechanical properties, low cost and low production cost
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Embodiment 1
[0039] Add 1g of sodium oxalate, 20g of caprolactam, 5g of sodium hydroxide, 130g of 60% sodium sulfide and 500g of DMPU into a reaction kettle with a nitrogen inlet and outlet, a water separator, a stirrer and a thermometer, under nitrogen protection, at a temperature of 200 ℃ dehydration reaction for 0.5 hours, lower the temperature to 160 ℃ and then add 113.9g p-difluorobenzene (0.999mol) and 0.462g halogenated aromatic compound (0.0005mol bi(4-p-fluorophenoxydiphenyl sulfone)+0.0005mol 1 , 4-dibromo-3-chlorobenzene), react at a temperature of 180°C for 1 hour, then keep at a temperature of 200°C for 8 hours, flash the reaction liquid to recover a part of the solvent, and then heat filter the polymer slurry to separate and polymerize material and solvent, collect the solid polymer, wash it with tap water, dry it and then purify it with deionized water and acetone, and dry it at a temperature of 100°C and a vacuum of 0.09MPa for 24 hours to obtain an ultra-high molecular weig...
Embodiment 2
[0042] 10g Lithium Acetate, 1g6-aminocaproic acid, 10g Potassium Hydroxide, 130g and 300gDMI containing 60% sodium sulfide are added in the reactor with nitrogen inlet and outlet, water separator, stirrer and thermometer, under nitrogen protection, Dehydration reaction at 180°C for 1 hour, cooling to 180°C and then adding 139.7g p-dichlorobenzene (0.95mol) and 19.31g halogenated aromatic compound (0.04mol bis(p-chlorophenoxy)benzophenone + 0.01mol 2,5-dichlorobenzoic acid), reacted at 260°C for 3 hours, then kept at 280°C for 1 hour, flashed the reaction solution to recover a part of the solvent, and then filtered the polymer slurry to separate the polymer and solvent, collect the solid polymer, wash it with tap water, dry it, then purify it with deionized water and acetone, and dry it at a temperature of 120°C under a vacuum of 0.07MPa for 24 hours to obtain an ultra-high molecular weight polyarylene sulfide extrusion grade resin B . Use α-chloronaphthalene as a solvent to p...
Embodiment 3
[0045] Add 5g of trisodium phosphate, 10g of polyethylene glycol-600, 0.1g of potassium hydroxide, 130g of 60% sodium sulfide and 200g of N-methylpyrrolidone into the reaction with nitrogen inlet and outlet pipes, water separator, stirrer and thermometer In the still, under the protection of nitrogen, dehydration reaction was carried out at a temperature of 160°C for 4 hours, and then 233.6g p-dibromobenzene (0.99mol) and 2.15g halogenated aromatic compound (0.002mol bis(p-bromophenoxy ) diphenyl sulfone + 0.008mol 2 ,5-difluoroaniline), react at a temperature of 230°C for 6 hours, and then keep at a temperature of 260°C for 6 hours, flash the reaction liquid to recover a part of the solvent, and then carry out the polymer slurry Heat filtration to separate the polymer and solvent, collect the solid polymer, wash it with tap water, dry it and then purify it with deionized water and acetone, dry it at a temperature of 80°C and a vacuum of 0.08 MPa for 8 hours to obtain ultra-hig...
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